超声波萃取-高效液相色谱-串联质谱同时测沉积物中10种PPCPs化合物

基于EPA1694方法,应用超声波萃取-高效液相色谱-串联质谱技术,建立了沉积物中对乙酰氨基酚、林可霉素、甲氧苄啶、咖啡因、阿奇霉素、磺胺甲唑、泰乐菌素、地尔硫卓、卡马西平及氟西汀等10种药物和个人护理品(PPCPs)的分析检测方法。样品经超声萃取、离心和SAX阴离子交换柱净化,以高效液相色谱-串联质谱仪多反应监测(MRM)模式进行离子定性、定量分析。10种药物加标回收率实验结果表明:添加低浓度样品20 ng/g,回收率为61.1%~128.5%,相对标准偏差(RSD)为1.7%~17.5%(n=5);添加高浓度样品400 ng/g,回收率为66.4%~126.7%,RSD为2.3%~18.0%(n=5),最低检测限为0.12~4.46 ng/g。该方法具有检测限低和回收率高的特点,并经实际样品验证发现,该方法适用于检测沉积物中10种PPCPs化合物。

Simultaneous Determination of 10 PPCPs in Sediments Using Ultrasound Extraction and HPLC-MS/MS

A method for the simultaneous determination of ten pharmaceutical and personal care products (PPCPs) (acetaminophen, lincomycin, trimethoprim, caffeine, azithromycin, sulfamethoxazole, tylosin, diltiazem, carbamazepine and fluoxetine) in sediments using liquid chromatography-tandem mass spectrometric was established. Samples were first extracted with ultrasonic, then cleaned up by solid phase extraction, and finally determined by tandem mass spectrometry with MRM mode. Recoveries were within 61.1%-128.5% and 66.4%-126.7% at the spiked level of 20 ng/g and 400 ng/g, respectively. The relative standard deviations (RSD, n=5) for the ten PPCPs were 1.7%-17.5% at 20 ng/g and 2.3%-18.0% at 400 ng/g. The detection limits ranged from 0.12-4.46 ng/g for ten PPCPs. The method has been successfully applied to the survey of selected ten PPCPs in sediments from Tuhai and Duliujian River, China.